CN104725670B - Phenol red or derivatives thereof intercalation ultraviolet blocking material of a kind of supramolecular structure and preparation method thereof - Google Patents
Phenol red or derivatives thereof intercalation ultraviolet blocking material of a kind of supramolecular structure and preparation method thereof Download PDFInfo
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- CN104725670B CN104725670B CN201510131813.9A CN201510131813A CN104725670B CN 104725670 B CN104725670 B CN 104725670B CN 201510131813 A CN201510131813 A CN 201510131813A CN 104725670 B CN104725670 B CN 104725670B
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Abstract
The invention discloses phenol red or derivatives thereof intercalation ultraviolet blocking material of a kind of supramolecular structure and preparation method thereof.The technical scheme is that：Using nitrate anion Intercalated as precursor, phenol red or derivatives thereof molecule is inserted into by nitrate anion Intercalated precursor interlayer using ion-exchange, assembling obtains that crystal phase structure is good, the phenol red Intercalated of excellent performance.Phenol red or derivatives thereof the intercalation ultraviolet blocking material of supramolecular structure prepared by the present invention is higher than 95% to the ultraviolet-resistant rate of 220 400nm wave bands, with excellent ultraviolet-resistant performance, has expanded the scope of ultraviolet isolating agent；The heat endurance of the material is good, and temperature of initial decomposition has brought up to 340 DEG C, is a kind of excellent optothermal stabilizer；It can increase substantially the ability of its anti-ultraviolet ageing as the additive of pitch, plastics, rubber Polymer material with phenol red or derivatives thereof the intercalation ultraviolet blocking material of the supramolecular structure for preparing of the present invention, increase the service life.
Description
Technical field：
The invention belongs to inorganic functional material technical field, more particularly to a kind of supramolecular structure is phenol red or derivatives thereof inserts
Layer ultraviolet blocking material and preparation method thereof.
Background technology：
Environmental pollution brings increasing considerably for ultraviolet, because of the photochemical effect and biological effect produced by ultraviolet
Very significantly, cause pitch and other macromolecule polymeric material agings, cause the reduction of its performance, viscosity increase, softening point liter
It is high, it is therefore necessary to study efficient uvioresistant additive.Phenol red English name is phenolsulfonphthalein, letter
PSPT is written as, there is certain uv absorption property in 220~400nm wave bands, outward appearance is deep red crystalline powder, difficult at room temperature
Water is dissolved in, is dissolved in NaOH solution, is a kind of more common pH value of solution indicator.PSPT is easily decomposed at relatively high temperatures, so
Limit its application and using effect.
Hydrotalcite (Layered Double Hydroxides, be abbreviated as LDHs) is the important novel inorganic function of a class
Material, the intercalation assembling property having using hydrotalcite and good photo and thermal stability, have as additive or carrier
Very high application value.
The content of the invention：
It is an object of the invention to provide a kind of supramolecular structure phenol red or derivatives thereof intercalation ultraviolet blocking material and its system
Preparation Method.
The technical scheme is that：, will be phenol red using ion-exchange using nitrate anion Intercalated as precursor
Or derivatives thereof be inserted into nitrate anion Intercalated precursor interlayer, it is good, excellent performance that assembling obtains crystal phase structure
Phenol red Intercalated.
Phenol red or derivatives thereof the intercalation ultraviolet blocking material of supramolecular structure of the present invention, its chemical formula is [Mg2+ 1- xAl3+ x(OH)2]x+(A2-)x/2·mH2O, wherein x are Al3+/(Mg2++Al3+) material the ratio between amount, 0.28≤x≤0.39；M is
Interlayer crystalline water molecules number, 0.9≤m≤1.2；A2-For phenol red or derivatives thereof ion.
Phenol red or derivatives thereof the specific preparation process of intercalation ultraviolet blocking material of supramolecular structure of the present invention is：
A. compound concentration is 0.02-0.2mol/L nitrate anion Intercalated precursor suspension；
B. it is dissolved in removing CO by phenol red or derivatives thereof2Deionized water in be configured to concentration for 0.04-0.4mol/L
Solution, it is 11-12 to adjust solution ph with NaOH；
C. under nitrogen protection, step B solution is added in step A suspension and quickly mixed, it is phenol red or its spread out
Biological is (1-4) with nitrate anion mole ratio in nitrate anion Intercalated precursor:1, under nitrogen protection, quick stirring,
At a temperature of 60-100 DEG C, preferably 80-95 DEG C, crystallization 8-14 hours, filtering, washing, be dried to obtain supramolecular structure it is phenol red or
Its derivative intercalation ultraviolet blocking material.
The structural formula of described nitrate anion Intercalated precursor is [Mg2+ 1-xAl3+ x(OH)2]x+(NO3 -)x·
mH2O, wherein x are Al3+/(Mg2++Al3+) material the ratio between amount, 0.29≤x≤0.35；M is interlayer crystalline water molecules number, 0.7
≤m≤1.2。
Phenol red or derivatives thereof the intercalation ultraviolet blocking material of the above-mentioned supramolecular structure prepared is used as the ultraviolet resistance of pitch
Every the application of agent.
The beneficial effects of the invention are as follows：
1. phenol red or derivatives thereof anion is inserted hydrotalcite layers by the present invention, the distinctive space confinement of hydrotalcite is utilized
Effect, makes phenol red or derivatives thereof the conformation in hydrotalcite layers change, sets up the big conjugated system of full molecule, conjugacy
Increase cause phenol red or derivatives thereof the absorption to ultraviolet to obtain a certain degree of enhancing, expand absorption region,
Excellent uv absorption property is produced, with reference to the uv-shielding capacity of neatly stone veneer in itself, makes the material that there is excellent purple
Outer barrier property；
2. intercalation has prepared the phenol red intercalated houghite material that interlayer anion is divalence to the present invention first, and phenol red
Price is less than common ultraviolet absorber, and this provides possibility for large-scale application；
3. phenol red or derivatives thereof the intercalation ultraviolet blocking material of supramolecular structure prepared by the present invention is to 220-400nm wave bands
Ultraviolet-resistant rate be higher than 95%, with excellent ultraviolet-resistant performance.Simultaneously after intercalation, by the decomposition temperature of object from 214
DEG C lifting is to 340 DEG C, and product has higher heat endurance, has expanded the scope of ultraviolet isolating agent；
4. with phenol red or derivatives thereof intercalation ultraviolet blocking material the adding as pitch of the supramolecular structure for preparing of the present invention
Plus agent can increase substantially the ability of its anti-ultraviolet ageing, extend pitch service life.
Brief description of the drawings
Fig. 1 is MgAl-PSPN-LDHs prepared by embodiment 1 XRD spectra.
Fig. 2 is phenol red TG-DTA spectrograms.
Fig. 3 is MgAl-PSPN-LDHs prepared by embodiment 1 TG-DTA spectrograms.
Fig. 4 is the ultraviolet reflectance spectrogram of embodiment 1, wherein：A is nitrate anion Intercalated precursor, and b is phenol red, c
It is MgAl-PSPN-LDHs.
Fig. 5 is the ultraviolet reflectance spectrogram of embodiment 4, wherein：A is cresol red, and b is MgAl-CPSPN-LDHs.
Embodiment
Embodiment 1：
Step A：By 30.72g (0.12mol) solid Mg (NO3)2·6H2O and 22.51g (0.06mol) solid Al
(NO3)3·9H2O, is dissolved in except CO2Deionized water in, be configured to 150mL mixing salt solution；14.4g NaOH is weighed, it is molten
In except CO2In deionized water, 150mL aqueous slkalis are made into；Two kinds of solution are added into rotation film reaction with identical flow velocity at room temperature
Obtained slurries are moved to 500mL flasks by fast nucleation in device, 80 DEG C of crystallization 8 hours, and centrifuge washing is about 7,60 DEG C to pH
Dry 12 hours, obtain nitrate anion Intercalated precursor, its structural formula is Mg0.64Al0.36(OH)2(NO3 -)0.36·
0.9H2O；
Take above-mentioned product 22.81g (0.01molNO3 —) in three-necked flask with removing CO2Deionized water ultrasonic disperse, match somebody with somebody
75mL suspension is made；
Step B：The phenol red 75mL that are dissolved in of 7.09g (0.02mol) are weighed except CO2Deionized water in, under rapid mixing conditions
About 0.03gNaOH is added, regulation solution ph is 11-12；
Step C：Under nitrogen protection, step B solution is added in step A suspension and quickly mixed, nitrate anion
Nitrate anion and phenol red mol ratio are 1 in Intercalated precursor:2, crystallization 14 hours at 80 DEG C are centrifuged, with removing
CO2Deionized water to wash to pH be about 7,60 DEG C of dryings 12 hours, obtain the phenol red intercalation ultraviolet blocking material of supramolecular structure,
It is designated as MgAl-PSPN-LDHs.
Obtained product is subjected to the sign such as XRD, IR, elementary analysis and show that its chemical formula is Mg0.60Al0.39(OH)2
(A2-)0.18·H2O, A2-For phenol red anion.
By X-ray powder diffraction (XRD), infrared (IR), elemental analysis, show that phenol red anion has been assembled into
Hydrotalcite layers simultaneously there occurs conformation change.TG-DT A spectrum (TG-DSC) result carried out to it is shown in Fig. 1, Fig. 2, as a result table
The temperature of initial decomposition of its bright intercalation product is 340 DEG C, and the temperature of initial decomposition than PSPN improves a lot.With UV, visible light point
The ultraviolet reflectance curve that analysis method is determined is shown in Fig. 3, finds out that its ultraviolet isolating rate to 220-400 wavelength bands is higher than by Fig. 3
95%.
PSPN/BN, MgAl-PSPN-LDHs/BN sample mould and pure BN (pitch) sample mould is respectively prepared by addition 3wt%.
After being irradiated 4 days to sample mould in ultraviolet accelerated ageing case, the viscosity and softening point of 3 samples after pre-irradiation are surveyed respectively.Pure BN
120 DEG C of viscosity before and after aging increase to 1.190Pas, viscosity aging index by 0.860PasFor 38.4；Before and after PSPN/BN agings 120 DEG C of viscosity by
1.30Pas increases to 1.531Pas, VAI=17.8；Before and after MgAl-PSPN-LDHs/BN agings 120 DEG C of viscosity by
0.913Pas increases to 0.988Pas, VAI=8.2；Softening point before and after pure BN agings increases to 50.1 DEG C by 45.6 DEG C,
S=4.5 DEG C of value added Δ, softening point increases to 50.5 DEG C, S=3.1 DEG C of Δ, MgAl- by 47.4 DEG C before and after PSPN/BN agings
Softening point increases to 47.2 DEG C, S=1.2 DEG C of Δ by 46 DEG C before and after PSPN-LDHs/BN agings.Add MgAl-PSPN-LDHs's
Pitch has more excellent anti-ultraviolet ageing performance.
Embodiment 2：
Step A：Nitrate anion Intercalated precursor suspension is prepared, method is identical with step A in embodiment 1；
Step B：The phenol red 75mL that are dissolved in of 3.55g (0.01mol) are weighed except CO2Deionized water in, under rapid mixing conditions
About 0.03gNaOH is added, regulation solution ph is 11-12；
Step C：Under nitrogen protection, step B solution is added in step A suspension and quickly mixed, nitrate anion
Nitrate anion and phenol red mol ratio are 1 in Intercalated precursor:1, crystallization 8 hours at 90 DEG C are centrifuged, with removing
CO2Deionized water to wash to pH be about 7,60 DEG C of dryings 12 hours, obtain the phenol red intercalation ultraviolet blocking material of supramolecular structure,
It is designated as MgAl-PSPN-LDHs.
Obtained product is subjected to the sign such as XRD, IR, elementary analysis and show that its chemical formula is Mg0.61Al0.36(OH)2
(A2-)0.17·1.2H2O, A2-For phenol red anion.
MgAl-PSPN-LDHs initial decomposition temperature is 340 DEG C, and the ultraviolet-resistant rate to 220-400nm wave bands is higher than
95%.
Embodiment 3：
Step A：Nitrate anion Intercalated precursor suspension is prepared, method is identical with step A in embodiment 1；
Step B：The phenol red 75mL that are dissolved in of 14.18g (0.04mol) are weighed except CO2Deionized water in, under rapid mixing conditions
About 0.03gNaOH is added, regulation solution ph is 11-12；
Step C：Under nitrogen protection, step B solution is added in step A suspension and quickly mixed, nitrate anion
Nitrate anion and phenol red mol ratio are 1 in Intercalated precursor:4, crystallization 14 hours at 95 DEG C are centrifuged, with removing
CO2Deionized water to wash to pH be about 7,60 DEG C of dryings 12 hours, obtain the phenol red intercalation ultraviolet blocking material of supramolecular structure,
It is designated as MgAl-PSPN-LDHs.
Obtained product is subjected to the sign such as XRD, IR, elementary analysis and show that its chemical formula is Mg0.63Al0.35(OH)2
(A2-)0.17·0.9H2O, A2-For phenol red anion.
MgAl-PSPN-LDHs initial decomposition temperature is 345 DEG C, and the ultraviolet-resistant rate to 220-400nm wave bands is above
95%.
Embodiment 4：
Step A：Nitrate anion Intercalated precursor suspension is prepared, method is identical with step A in embodiment 1；
Step B：Weigh 15.30g (0.04mol) o-cresol red and be dissolved in 75mL except CO2Deionized water in, quick stirring bar
About 0.03gNaOH is added under part, regulation solution ph is 11-12；
Step C：Under nitrogen protection, step B solution is added in step A suspension and quickly mixed, nitrate anion
Nitrate anion and o-cresol red mol ratio are 1 in Intercalated precursor:4, crystallization 14 hours at 80 DEG C are centrifuged,
With removing CO2Deionized water to wash to pH be about 7,60 DEG C of dryings 12 hours, obtain supramolecular structure o-cresol red intercalation ultraviolet
Barrier material, is designated as MgAl-CPSPN-LDHs.
Obtained product is subjected to the sign such as XRD, IR, elementary analysis and show that its chemical formula is Mg0.61Al0.37(OH)2
(A2-)0.16·0.9H2O, A2-For o-cresol red anion.
MgAl-CPSPN-LDHs is above 95% to the ultraviolet-resistant rate of 220-400nm wave bands.
Embodiment 5：
Step A：By 46.08g (0.15mol) solid Mg (NO3)2·6H2O and 22.51g (0.06mol) solid Al
(NO3)3·9H2O, is dissolved in except CO2Deionized water in, be configured to 150mL mixing salt solution；16.8gNaOH is weighed, is dissolved in
Except CO2In deionized water, 150mL aqueous slkalis are made into；Two kinds of solution are added into rotation membrane reactor with identical flow velocity at room temperature
Obtained slurries are moved to 500mL flasks by middle fast nucleation, 80 DEG C of crystallization 8 hours, and centrifuge washing is about 7,60 DEG C to pH and done
Dry 12 hours, nitrate anion Intercalated precursor is obtained, its structural formula is Mg0.71Al0.29(OH)2(NO3 -)0.29·
0.8H2O；
Take above-mentioned product 26.09g (0.01molNO3 —) in three-necked flask with removing CO2Deionized water ultrasonic disperse, match somebody with somebody
75mL suspension is made；
Step B：The phenol red 75mL that are dissolved in of 7.09g (0.02mol) are weighed except CO2Deionized water in, under rapid mixing conditions
About 0.03gNaOH is added, regulation solution ph is 11-12；
Step C：Under nitrogen protection, step B solution is added in step A suspension and quickly mixed, nitrate anion
Nitrate anion and phenol red mol ratio are 1 in Intercalated precursor:2, crystallization 8 hours at 80 DEG C are centrifuged, with removing
CO2Deionized water to wash to pH be about 7,60 DEG C of dryings 12 hours, obtain the phenol red intercalation ultraviolet blocking material of supramolecular structure,
It is designated as MgAl-PSPN-LDHs.
Obtained product is subjected to the sign such as XRD, IR, elementary analysis and show that its chemical formula is Mg0.70Al0.29(OH)2
(A2-)0.15·1.1H2O, A2-For phenol red anion.
MgAl-PSPN-LDHs initial decomposition temperature is 343 DEG C, and the ultraviolet-resistant rate to 220-400nm wave bands is higher than
95%.
Embodiment 6：
Step A：Nitrate anion Intercalated precursor suspension is prepared, method is identical with step A in embodiment 5；
Step B：The phenol red 75mL that are dissolved in of 3.55g (0.01mol) are weighed except CO2Deionized water in, under rapid mixing conditions
About 0.03gNaOH is added, regulation solution ph is 11-12；
Step C：Under nitrogen protection, step B solution is added in step A suspension and quickly mixed, nitrate anion
Nitrate anion and phenol red mol ratio are 1 in Intercalated precursor:1, crystallization 14 hours at 95 DEG C are centrifuged, with removing
CO2Deionized water to wash to pH be about 7,60 DEG C of dryings 12 hours, obtain the phenol red intercalation ultraviolet blocking material of supramolecular structure,
It is designated as MgAl-PSPN-LDHs.
Obtained product is subjected to the sign such as XRD, IR, elementary analysis and show that its chemical formula is Mg0.72Al0.28(OH)2
(A2-)0.11·1.2H2O, A2-For phenol red anion.
MgAl-PSPN-LDHs initial decomposition temperature is 341 DEG C, and the ultraviolet-resistant rate to 220-400nm wave bands is higher than
95%.
Embodiment 7：
Step A：Nitrate anion Intercalated precursor suspension is prepared, method is identical with step A in embodiment 5；
Step B：The phenol red 75mL that are dissolved in of 14.18g (0.04mol) are weighed except CO2Deionized water in, under rapid mixing conditions
About 0.03gNaOH is added, regulation solution ph is 11-12；
Step C：Under nitrogen protection, step B solution is added in step A suspension and quickly mixed, nitrate anion
Nitrate anion and phenol red mol ratio are 1 in Intercalated precursor:4, crystallization 10 hours at 90 DEG C are centrifuged, with removing
CO2Deionized water to wash to pH be about 7,60 DEG C of dryings 12 hours, obtain the phenol red intercalation ultraviolet blocking material of supramolecular structure,
It is designated as MgAl-PSPN-LDHs.
Obtained product is subjected to the sign such as XRD, IR, elementary analysis and show that its chemical formula is Mg0.69Al0.32(OH)2
(A2-)0.14·0.9H2O, A2-For phenol red anion.
MgAl-PSPN-LDHs initial decomposition temperature is 339 DEG C, and the ultraviolet-resistant rate to 220-400nm wave bands is higher than
95%.
Embodiment 8：
Step A：Nitrate anion Intercalated precursor suspension is prepared, method is identical with step A in embodiment 5；
Step B：Weigh 3.82g (0.01mol) o-cresol red and be dissolved in 75mL except CO2Deionized water in, quick stirring bar
About 0.03gNaOH is added under part, regulation solution ph is 11-12；
Step C：Under nitrogen protection, step B solution is added in step A suspension and quickly mixed, nitrate anion
Nitrate anion and o-cresol red mol ratio are 1 in Intercalated precursor:1, crystallization 8 hours at 95 DEG C are centrifuged, and are used
Except CO2Deionized water to wash to pH be about 7,60 DEG C of dryings 12 hours, obtain the ultraviolet resistance of supramolecular structure o-cresol red intercalation
Barrier material, is designated as MgAl-CPSPN-LDHs.
Obtained product is subjected to the sign such as XRD, IR, elementary analysis and show that its chemical formula is Mg0.69Al0.30(OH)2
(A2-)0.14·1.2H2O, A2-For o-cresol red anion.
MgAl-CPSPN-LDHs is higher than 95% to the ultraviolet-resistant rate of 220-400nm wave bands.
Claims (4)
1. a kind of phenol red intercalation ultraviolet blocking material of supramolecular structure, it is characterised in that its chemical formula is [Mg2+ 1-xAl3+ x
(OH)2]x+(A2-)x/2·mH2O, wherein x are Al3+/(Mg2++Al3+) material the ratio between amount, 0.28≤x≤0.39；M is interlayer knot
Brilliant moisture subnumber, 0.9≤m≤1.2；A2-For phenol red ion.
2. the preparation method of the phenol red intercalation ultraviolet blocking material of supramolecular structure according to claim 1, it is characterised in that
Its specific preparation process is：
A. compound concentration is 0.02-0.2mol/L nitrate anion Intercalated precursor suspension；
B. it is dissolved in removing CO by phenol red2Deionized water in be configured to concentration be 0.04-0.4mol/L solution, adjusted with NaOH
Solution ph is 11-12；
C. under nitrogen protection, step B solution is added in step A suspension and quickly mixed, it is phenol red to be inserted with nitrate anion
Nitrate anion mole ratio is (1-4) in layer magnalium hydrotalcite precursor:1, under nitrogen protection, quick stirring, in 60-100 DEG C of temperature
Under, crystallization 8-14 hours, filtering, washing are dried to obtain the phenol red intercalation ultraviolet blocking material of supramolecular structure.
3. preparation method according to claim 2, it is characterised in that described nitrate anion Intercalated precursor
Structural formula is [Mg2+ 1-xAl3+ x(OH)2]x+(NO3 -)x·mH2O, wherein x are Al3+/(Mg2++Al3+) material the ratio between amount, 0.29
≤x≤0.35；M is interlayer crystalline water molecules number, 0.7≤m≤1.2.
4. the phenol red intercalation ultraviolet blocking material conduct of the supramolecular structure prepared according to the method in claim 2 or 3
The application of pitch ultraviolet-resistant agent.
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| CN110511579A (en) * | 2019-08-01 | 2019-11-29 | 中交上海港湾工程设计研究院有限公司 | A kind of ageing-resistant asphalt modifier and preparation method thereof and ageing-resistant pitch |
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| CN1850787A (en) * | 2006-05-19 | 2006-10-25 | 北京化工大学 | Supermolecular intercalation 2-phenylbenzimidazole-5-sulfonic acid, and its preparing method and use |
| CN102180614A (en) * | 2011-03-21 | 2011-09-14 | 北京化工大学 | Magnelium base layer-shaped double-hydroxide ultraviolet barrier material used in anti-aging asphalt |
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| CN1850787A (en) * | 2006-05-19 | 2006-10-25 | 北京化工大学 | Supermolecular intercalation 2-phenylbenzimidazole-5-sulfonic acid, and its preparing method and use |
| CN102180614A (en) * | 2011-03-21 | 2011-09-14 | 北京化工大学 | Magnelium base layer-shaped double-hydroxide ultraviolet barrier material used in anti-aging asphalt |
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